Veba-Chemie Aktiengesellschaft

Chemische Werke Huls Aktiengesellschaft

Huls Aktiengesellschaft

August Sommer

Rainer Brucker

Wilhelm Heitmann

Martin Urban

Richard Wessendorf

Heinrich Birkelbach

Norbert Wozny

Dietrich Schlueter

A method of manufacturing a catalyst for hydration of olefins to alcohols. A montmorillonite-containing clay is employed as a catalyst support for phosphoric acid, to which a fine-grained silica gel is added after a first acid treatment. The silica gel has a particle size distribution between 30 and 60 micron, a pore volume of 0.9-1.7 ml/g, and a specific surface of 200-500 sq m/g.

Method of manufacturing a catalyst for hydration of olefins to alcohols

A distillation process for the production of dehydrated ethanol from dilute aqueous solutions of ethanol characterized in that the distillation is performed in a two-column system wherein the first column--for rectification--is operated under such a pressure that the second column--for dehydration--is heated exclusively with the vapors of the first column; in the first column the concentration of the dilute aqueous ethanol is effected to an ethanol concentration below the composition of the binary ethanol-water azeotrope; the separation of water is effected from the lower layer of the condensed head product of the second column; the separation of impurities and entrainers, having a lower boiling point than ethanol, is effected at the head of the first column and that of impurities, having a higher boiling point, above the feed point of the dilute aqueous solution in the first column; and, in the second column, the dehydration is effected by means of entrainers, with the addition of a fuel component or fuel, to which the ethanol is to be added, if required, while separating the aqueous phase as a head product.

Distillation process for the production of dehydrated ethanol

A method for producing a carrier for a catalyst comprising the steps of mixing solutions of a soluble salt of aluminum and a soluble salt of silicic acid in a ratio that gives a precipitate comprising aluminum silicate having a weight ratio of Al.sub.2 O.sub.3 :SiO.sub.2 of 1:5 to 1:7, forming the precipitate into a carrier body, consolidating the carrier body by heating, and contacting the carrier body with an acid to reduce the Al.sub.2 O.sub.3 content to 1-5%. Thus produced carrier bodies are useful for catalyzing the hydration of olefins to alcohols when impregnated with phosphoric acid.

Method for producing a catalyst for the hydration of olefins

A method is disclosed of preparing alcohols having 2 to 4 carbon atoms by catalytic hydration of the corresponding olefins on acid catalysts at elevated temperature and elevated pressure, characterized in that byproducts of the hydration, namely corresponding ethers and/or low-polymerized hydrocarbons and/or undesired alcohols, which form upon the passage of the input product through catalyst bed, are fed to the input product before entry into the reactor, said method being characterized in that:

Method of preparing alcohols having two to four carbon atoms by

A method for producing a catalyst comprising phosphoric acid and a carrier, for the hydration of olefins with 2-3 carbon atoms to the corresponding alcohols, the method comprising:

Method of producing a catalyst from clay minerals for the hydration of

A process for producing a clay-containing catalyst for the hydration of olefins having 2-3 carbon atoms into alcohols, which comprises: (A) acid-treating a montmorillonite-containing clay which is contaminated by not more than 3% of quartz, feldspar or mica, and which may contain up to 0.5% of K.sub.2 O, until the clay has an Al.sub.2 O.sub.3 content of 13-18% by weight, thereby obtaining a surface area of 200-400 m.sup.2 /g; (B) molding the clay at a total water content of 20-35%; (C) calcining at 500.degree.-800.degree. C.; (D) acid-treating the molded and calcined clay to an Al.sub.2 O.sub.3 content of 1-5% by weight, thereby obtaining a surface area of 150-250 m.sup.2 /g; and (E) impregnating said material with phosphoric acid.

Process for the production of a catalyst for the hydration of olefins

A process for the hydration of olefins to prepare alcohol is disclosed, the hydration being effected in the presence of a phosphorus acid-containing catalyst. There is disclosed a process in which vaporized phosphoric acid is admixed with a gas mixture before the same is added to the reactor, the phosphoric acid being in an amount corresponding to the amount of phosphoric acid discharged during the hydration. In such amount the process can be carried out without further phosphoric acid addition.

Hydration of olefins using vaporized phosphoric acid

An improvement in a process for refining crude glyoxal solutions, especially those obtained by the oxidation of acid aldehyde with nitric acid, wherein the crude glyoxal solution, free of volatile acids, is neutralized, the glyoxal is transformed to the glyoxal semiacetal with an alcohol having 1 to 3 carbon atoms and, after separation of the salts and other impurities, is again hydrolized with water at elevated temperatures. The improvement described involves continuously extracting the glyoxal semiacetal formed with an organic solvent which is immiscible with water, hydrolyzing the extracted glyoxal semiacetal and refining the aqueous glyoxal solution obtained with active charcoal.

Continuous process for refining glyoxal

Crude glyoxal solutions obtained for example by the oxidation of acetaldehyde with nitric acid are purified by removing volatile acids followed by neutralization. Thereafter, the glyoxal is converted into a glyoxal glyoxal-di-(alkylhemiacetal) with an alcohol containing 1 to 3 carbon atoms with water removal during the conversion. After separating salts and other impurities, the glyoxal-di-(alkylhemiacetal) is hydrolyzed with water at elevated temperatures to yield pure glyoxal hydrate.

Process for purifying glyoxal

A water-free mixture of isopropyl alcohol, diisopropyl alcohol, diisopropyl ether and by-products is made by the catalytic hydration of propylene in the gaseous phase at temperatures of 140.degree.-170.degree.C under pressures of 25-40 atmospheres gauge. A water-to-propylene molar ratio of 0.1 to 0.25:1 is maintained in the hydration reaction. The crude product from the hydration reaction is dehydrated or dewatered in two columns without using a foreign withdrawing agent. Instead, diiosopropyl ether formed in the process itself is utilized as the withdrawing agent which is subsequently added to the water-free mixture together with additionally formed by-products. The water-free mixture formed according to the process can be used directly as an additive to gasoline fuel for motor vehicles.

Extractive distillation of isopropyl alcohol with an ether solvent

Olefins having two and three carbon atoms are hydrated in the presence of phosphoric acid-containing supported catalysts to the corresponding alcohols. For the hydration of olefins having two carbon atoms, the molar ratio of water to olefin is in the range of about 0.1-0.3 : 1, the reaction temperatures in the range of about 190.degree.-230.degree.C, and the reaction pressure is in the range of about 60-80 atmospheres gauge. For the hydration of olefins having three carbon atoms, the molar ratio of water to olefin is in the range of about 0.1-0.3 : 1, the reaction temperatures in the range of about 140.degree.-170.degree.C and the reaction pressure is in the range of about 20-45 atmospheres gauge. The only by-products which form in addition to the raw alcohol under these conditions are steam-volatile (water soluble) by-products which are separated from the raw alcohol in a washing extraction zone. The by-products are recycled in aqueous solution without organic phase to the hydration in the state in which they are producted at the top of the washing extraction zone after separating unreacted olefin.

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Herne, Germany

August Sommer